Measurement and Analysis facilities in Nanolab · – Light diffusion measurement: Candela CS10...
Transcript of Measurement and Analysis facilities in Nanolab · – Light diffusion measurement: Candela CS10...
UNIVERSITEIT TWENTE.
Measurement and Analysis
facilities in Nanolab
“Inside and outside the cleanroom”
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Contents
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Typical facilities
Available equipment by application
Resolution versus detection limit
Information depth, including depth profiles
Techniques used for analysis and characterization
Measurement and analysis techniques available in Nanolab
State of affairs for sample control
Visual inspection and optical microscopy
Thickness and optical properties
Roughness
Force Imaging
Homogenity
Electrical characterization
Wafer cleanliness
Scanning probe imaging
Contents mapping
Crystallinity
Thin layer contents
List of abbreviations
List of operators and supervisors
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Typical facilities
Inside the cleanroom a number of tools are present in order to inspect your
samples and decide whether your process was successful or not. Some of the
tools can also give an indication of the sample composition. The tools are used to
control dimensions of the samples produced .
• Length, width, depth/height, roughness, mass, homogeneity, hydrophobicity,
conductance and refractive index
In addition to the facilities in the cleanroom for inspection of your products we also
offer facilities for materials analysis and in particular surface analysis for members
of MESA+, other university members and people outside the university. We offer
equipment and expertise to prepare your samples for analysis. The equipment
can analyze bulk materials, but most techniques give information regarding to the
surface of materials, monolayers and thin films.
• Elemental content, crystal classes, crystal shape, directionality are a few of
the properties that can be measured. The sample dimensions can range from
a few nanometers to a few centimeters.
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Available equipment in alphabetical order of application
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Analysis of elemental contents
• Electron microscopes
• X-ray microscope
• X-ray diffractometers
Electrical Characterization
• 4 point probes
• EBIC
• Parameter Analyzer
Homogeneity
• Ellipsometers
• X-ray Photoelectron Spectrometer
Imaging
• Optical microscopes
• Electron microscopes
• Force microscope
Surface Energy Characterization
• Contact angle apparatus
Thickness
• Interferometer
• Ellipsometer
• Reflectometer
Topography
• Profilometer
• Force Microscope
Weight
• Balances
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Analysis Resolution versus detection limit for several techniques
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Surface analysis
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Surface analysis techniques
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Analysis Information depths given by the listed techniques, including
depth profiles
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Techniques used for materials analysis and characterization.
AES EDS GDMS SIMS TXRF XRFICP OES IGA
LA ICP MS LEXES RBS Raman FTIR GC MS
TOF SIMS
XPS ESCA XRD FIB OM SEM
SPM AFM
STEM TEM Ellipsometry XRF
Adhesion and bonding
Cleanliness
Thin layer analysis - Composition
Surface Analysis - Composition
Bulk Analysis - Composition
Particles - Contamination
Residues - Contamination
Discolorations - Contamination
Haze - Contamination
Layer - Contamination
Bulk - Contamination
Corrosion
Diffusion
Implant Profiles - Dopants
ULE Profiles - Dopants
Layers - Dopants
Two-dimensional Profiles - Dopants
Failure Analysis
Imaging/Mapping
Morphology
Topography
Profiling
Surface Chemistry
Thin Film Analysis
Present in MESA+
Chemical bonding / molecular information
Elemental information
Image information
Thickness and density information
Acknowledgement: Evans Analytical Group
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Topic of interestTechniques
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Measurement and analysis techniques found in the Nanolab and the MESA+ institute
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hν(IR)
hν(IR)
FTIR
1mm 10mm
0.0
1nm
5
00nm
hν(IR)
hν(x-ray)
hν(x-ray)
XRF
0.2μm 100mm
0.2
μm
1μ
m
CA
0.01°
0°
180°
Θ
droplet
hν(light)
hν(light)
Microscopy
0.2μm
0.2
μm
1m
m
hν(light)
Ellipsometry
1mm
0.0
1nm
5
00nm
Δ Ψ
EDX SEM
10nm-10μm
1nm
500nm hν
(x-ray)
e-
XPS
9μm
0.1
nm
5nm hν
(x-ray)
e-
photoelectron
Θ
hν(x-ray)
hν(x-ray)
XRD
0.2μm 100mm
0.2
μm
1m
m
SEM, EBSD, EBIC
1nm
1nm
500nm e-e-e-
A
AFM
2nm
1nm
100μ
m
hν(laser)
hν(ir-uv)
RAMAN
0.2μm
0.2
μm
1μ
m
Materials analysis
Imaging
Structural analysis
Information depth / height resolution
Spatial resolution
Nanolab / MESA+
EDX TEM
0.1nm 10nm
1nm
150nm hν
(x-ray)
e-
MP
25nm
0.5
nm
600μ
m
g
0μ
g
31g
Scales
3μg
?
4 point
1 mΩ/sq
10nm
1m
m I
V
FIB
15nm
10nm
1
0μ
m
e-e-
I+ X+
TEM
0.1nm
1nm
150nm
e-
e-
e-
stimulus
response
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State of affairs.
After each process step one could do an inspection of the products.
First controls should be the controls that do not change the state of the products.
Visual inspection, dust particles visible under light reflection
Optical microscopy inspection
– White light
– Yellow light
Layer thickness inspection, refractive index
– Non destructive
• Ellipsometer
• Reflectometer
• Interferometer
• Weighing scales
– Destructive
• Ball groover
Roughness measurement
– Mechanical profiling
– Scanning probe imaging
Homogenity
– Contact angle
– Ellipsometry for refractive index
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Further inspection and analysis
Electrical properties
– Square resistance
– I-V curves Imaging
– EBIC in Electron microscopy
Wafer cleanliness
– Light diffusion measurement: Candela CS10
Small scale imaging
– Scanning probe microscopy
• AFM
– Electron microscopy
• FIB
• SEM
• TEM
Contents analysis and mapping
– EDX for thick layer > 50 nm
– EELS for thin layers
– FTIR spectroscopy: transmissive or reflective
– XPS for thin layers < 5 nm
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Further inspection and analysis
Crystallography
– XRD for bigger sample > 5µm
– EBSD > 10 nm
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First control: Visual inspection and optical microscopy inspection
Visual inspection with help of a halogen cold light source can be done
in the SEM room. The light is also used as an illumination source
for the optical microscope in that room. The light in the SEM room
can be switched off for better dust/particle recognition
White light Optical microscopes from Olympus, Nikon, Leitz are
mostly used for visual inspection of whole wafers or smaller
samples to gain an impression of the product after a process step.
It can give a lot of information about the uniformity, the presence
of particle and process induced errors. Most metallurgical
microscopes are equipped with a camera to make digital images
and with software to measure
dimensions. Stereomicroscopes are used for quick inspection with
low a magnification on large samples.
Yellow light Fluorescence microscope, Nikon is used if structures are
made with fresh positive resist, not negative. The light will expose
the positive resist.
In the preparation room of the analysis group outside the cleanroom
there are a few microscopes to control the shape and roughness
of freshly prepared samples after polishing and to check samples
before carrying out electron microscopy.
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First control: Layer thickness inspection, refractive index
Non destructive
• Ellipsometers: A Woollam M-2000 spectroscopic ellipsometer
measures the change of polarization (in terms of Y and D)
upon reflection of incident light with the sample surface. The
films are measured over a wide wavelength range (245-1690 nm)
and at multiple incidence angles, allowing the accurate
determination of the film thickness and corresponding optical
constants (refractive index, extinction coefficient) for a wide range
of transparent and semi-transparent materials. The ellipsometer is
sensitive to less than a monolayer of material (sub-nm) on a
surface and is still able to determine film thicknesses up to tens of
micrometers. The llipsometer has a computer-controlled sample
stage for the determination of
variations in the layer thickness and optical constants
(refractive index, extinction coefficient) as a function of the
position on the sample.
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• Reflectometer: The thin film thickness mapping system, Filmetrics
F50 reflectometer, is based on measuring the reflectance of light
on a sample as function of wavelength, used to measure
homogeneous, partially absorbing, films with a thickness of more
than 50 nm. It is used to measure (semi) transparent films.
hν(light)
Ellipsometry
1mm
0.0
1nm
5
00nm
Δ Ψ
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First control: Layer thickness inspection, refractive index
• Non destructive
– The Bruker Contour GT-I Interferometer is a white light
interferometer, can be used to measure the topography
of a surface down to less than 1 nm. Lateral resolution is of
the order of 0.5 um.
– Weighing scales. The Sartorius ME36S OCE, is an analytical
micro balance.
It is an instrument to weigh small masses with very high
precision. The instrument is so precise that one has to
compensate for temperature, humidity and air buoyancy
changes to use it at its ultimate resolution and
reproducibility. The scales have a closed cabinet to control
the temperature and the air turbulence inside. It takes
some time for the balance to reach equilibrium in order to
make a good measurement. As an example; on a 4” silicon
wafer one can measure the increase of an oxide layer with 1
nm by measuring the weight gain of the wafer. This gain
would be around 11 μg for the change of 0.35 nm silicon in 1
nm silicon oxide.
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First control: Layer thickness inspection, refractive index
• Destructive
– Ball groover: A technique for determining the junction
depth of a P/N junction. Using a fast spinning ball a pit is
grinded into the test substrate and after staining the
substrate, using a microscope, the ring sizes can be
measured and these can be translated into junction depths.
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First control: Roughness measurement
Mechanical profilometers, scan a surface in a straight line with a small
needle. The needle follows the indentations and bumps of a
surface. The height differences can be made visible as a function
of distance. From this, the roughness is calculated. The needle of
the machine actually makes contact with the surface being
measured so it can damage the sample.
The Dektak 8 surface profiler is an advanced thin and thick step
height measurement tool capable of measuring steps down to 10
nm. Substrates up to five inches in dimension can be measured.
The Dektak 8 is especially setup up for doing fine measurements,
for this purpose it has a 2.5 μm stylus.
The Dektak 150 surface profiler is an advanced thin and thick step
height measurement tool capable of measuring steps down to 10
nm. Substrates up to five inches in dimension can be measured.
The Dektak 150 is especially setup up for doing stress
measurements, for this purpose it has a 12 μm stylus.
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First control: Roughness measurement
Scanning probe imaging
Atomic Force Microscope, Bruker ICON AFM: with a small probe
(tip, needle, pin, magnet) a sample can be imaged in quasi
contact or real contact mode. A monitored force is used to allow
the scanning tip follow the indentations or bumps of a sample.
Topography, magnetism, friction and other types of forces are
monitored with a computer. An image of the sample made for the
specific force is presented on a computer screen. As with a
profilometer, surface roughness can be calculated from the
measurements. The AFM is a setup for measurements in the
Scan Assist mode. The maximum step height is limited to 4 μm.
The depth resolution can be as small as 0.5 nm. The tip radius is
4 nm which is the maximum lateral resolution and the measuring
area has a maximum of 80 X 80 µm. Substrates with a
(maximum) diameter of 150 mm can be
measured.
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AFM
2nm
1nm
100
μm
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First control: Homogenity
Contact angle: The contact angle apparatus Dataphysics OCA 20
measures the hydrophobicity of a sample surface. The surface
tension of the fluid and/or the solid involved can be measured as
well as the surface homogeneity on a macroscopic scale. A tiny
drop
of a known fluid is put in contact with the sample surface under
controlled conditions like temperature and humidity. The angle
between the droplet and the surface is a measure for the surface
free energy.
Ellipsometry for refractive index homogenity: Woollam M-2000
mapping spectroscopic ellipsometer
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Further inspection and analysis: Electrical characterisation
• Square resistance:
– 4 point probe from Polytec. The four point probe is used
for automatic mapping of the sheet resistance of metals
and/or epitaxial layers and of doped silicon based
layers. A current is injected into a surface and extracted a
few millimeter further away. In between, the voltage over
a known distance is measured. From voltage and current,
the square resistance is calculated. Read out in Ω/sq. and
measuring range is from 1 mΩ/sq to 800 kΩ/sq. The
probe head is only suitable for metal layers up to 300 nm
and epitaxial layers
• I-V curves Imaging
– Parameter Analyser, HP
• EBIC in a scanning electron microscope, electron beam
induced current detector measures where the most electrons
are absorbed in a sample, i.e. where the conductivity is
highest
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Further inspection and analysis: Wafer cleanliness
KLA Tencor Candela CS10r Optical beam surface analyser
– > 80 micron particles
– Nano crystal defects
– Nanometer size scratches
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Further inspection: small scale imaging
Scanning probe imaging
Atomic Force Microscope, Bruker ICON AFM: with a small
probe (tip, needle, pin, magnet) a sample can be imaged in
quasi contact or real contact mode. A monitored force is used to
allow the scanning tip follow the indentations or bumps of a
sample. Topography, magnetism, friction and other types of
forces are monitored with a computer. An image of the sample
made for the specific force is presented on a computer screen.
As with a profilometer, surface roughness can be calculated from
the measurements. The AFM is a setup for measurements in the
Scan Assist mode. The maximum step height is limited to 4 μm.
The depth resolution can be as small as 0.5 nm. The tip radius is
4 nm which is the maximum lateral resolution and the measuring
area has a maximum of 80 X 80 µm. Substrates with a
(maximum) diameter of 150 mm can be
measured.
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AFM
2nm
1nm
100μ
m
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Further inspection: small scale imaging
Electron microscopy gives information on a much smaller scale than
the optical microscopes. There are 3 SEMs, 1 TEM and 1 FIB/SEM
directly accessible to customers of the Nanolab. There are a number
of groups that have their own electron microscopes.
Inside the cleanroom there are 2 SEMs available of which one can be
used for a first control of 4”wafers
JEOL JSM5610, with a tungsten tip source, for inspection of
large samples, up to 4” wafers. This is the first SEM one should
use. It is
easy to use and gives good results up to a magnification of
30000 x
FEI Sirion XL, a SEM, with a FEG (Field Emission Gun) source
and an in-lens detector, with higher resolution for inspection of
non-
magnetic small samples. It gives results up to a magnification of
150.000 x with a resolution of ~ 1.5 nm.
Because this SEM cannot hold 4”wafers, wafers have to be
parted to supply the smaller parts needed in this SEM.
These smaller samples can be brought closer to the SEM’s
objective lens and therefor be studied with lower energy
electrons. Charging can be less influential than in the JEOL SEM
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Further inspection and analysis: Small scale imaging
• Outside the cleanroom there are a couple of microscopes for
imaging and analysis.
• FEI NOVA600 Dual Beam combines Focused Ion Beam with
Scanning Electron Microscopy.
• The combination of these two techniques makes it ideal for
micromachining. Local etching with the ion-beam creates
structures suitable for cross-sectioning and TEM-sample
preparation in a predefined part of the substrate without
damaging other parts. Cross-sectioning reveals the
underlying structure imaged by SEM. TEM-sample
preparation thins the sample down to 100 nm with minimal
damage. A 16 bit pattern generator is available to create the
most amazing structures such as 3D Photonic Crystals.
Tungsten and platinum deposition is also available.
• For analysis there is the option of local etching of multi-
crystalline materials. It reveals not only the size of the
crystals but also differences in crystal orientation.
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FIB
15nm
10nm
1
0μ
m
e-e-
I+ X+
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Further inspection and analysis: Small scale imaging
– Zeiss Merlin SEM, with FEG tip and a number of different
detectors. This machine can reach an ultra high resolution
and is used for materials characterization and analysis. It is
operated by a dedicated operator who can obtain the best
results from your samples.
This High Resolution SEM is the workhorse in the analysis
laboratory. A microscope with a lateral resolution of approx. 1
nm. It can be used at both high and low electron
beam currents and high and low beam voltages which
allowsnon-conducting samples have to be investigated.
Next to the obligatory SEM images, detectors can yield
extra information about the sample. EDX will give the
elemental composition of the material down to a certain
depth. EBSD will give information about the crystal structure
and the crystal orientations on flat-polished samples. A STEM
detector produces TEM-like images in the SEM. The
resolution of this technique is of the order of 0.6 nm
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SEM, EBSD, EBIC
1nm
1nm
500nm e-e-e-
A
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Further inspection and analysis: Small scale imaging
– FEI (Philips) CM300ST-FEG TEM, with the highest
spatial resolution available at the university. Information
regarding size, elemental composition and crystal
structure of a sufficiently thin, prepared electronic
transparent specimen can be obtained. An expert
operator prepares the samples if necessary and operates
the microscope for best results.
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TEM
0.1nm
1nm
150nm
e-
e-
e-
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Further inspection and analysis: Contents mapping
Analysis tools are used to determine the chemistry of a sample. In the
nanolab, most of these tools are specialized in measuring the
composition of thin films and surfaces. Tools for measuring bulk
properties are essentially limited to optical instruments that
measure the optical properties of (semi) transparent materials.
– EDX for thick layer > 50 nm, detectors on SEM and TEM. The
lateral resolution is as good as the thickness of the X-ray
generation volume.
– EELS for thin layers, detector on TEM
– FTIR spectroscopy: transmissive or reflective optical respons
– XPS for thin layers < 5 nm but a very big lateral resolution >
10 µm
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Further inspection and analysis: Crystalinity and Contents
– XRD, X-Ray Diffractometers, from Panalytical is used to find
the atomic contents and possible crystal classes of small
crystals in a surface or in a powder.
Bruker
Philips XRD model Expert system II wafer characterization,
crystal plane distance measurements
XRD is used for relatively bigger samples > 5µm
– EBSD from HKL systems as an extra detector on the Zeiss
Merlin HRSEM. For the technique of Electron BackScatter
Diffraction one uses a SEM as a source of incident electrons
that are subsequently backscattered and diffracted by the
crystal lattice of small crystals that make up the surface The
information comes from a thin layer ~5 nm thick and gives
information about the crystal lattice parameters. Together
with EDX it can resolve the materials at a surface EBSD is
used for relative small and thin samples < 10 nm in height
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Further inspection and analysis: Crystallography
Transmission Electron Microscope. FEI (Philips) CM300ST for the
investigation of the internal structure of a material down to sub
nanometer dimensions. A number of detectors are mounted onto the
microscope to facilitate chemical analysis techniques. Chemical
information using EDX, EELS and EFTEM imagingdown to approx.
the nanometer scale.
Point resolution = 0.2 nm@300 kV, Line resolution = 0.14 nm
@300 kV.
Single atoms can not be observed with a TEM. But crystal planes and
distances between them can be resolved thereby giving
crystallographic information on a very small scale sample
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Further inspection and analysis: Homogenity and thin layer contents
• Scanning X-ray Photoelectron Spectrometer PHI Quantera XPS.
• Homogenity. In this machine we can map the photoelectron
electron escape probability from the surface of the sample.
The scanning x-ray electron images can show areas with less
or more brightness. The brightness is an indication of the
escape probability. Metallic samples show higher probabilities
and non conducting parts lower probabilities. Bright or dark
spots on homogenous wafers reveal inhomogeneities.
• Contents. XPS is also a technique to measure the contents of
very thin layers of materials. The lateral resolution of the
instrument is about 10 μm for structures with high contrast. It
is not comparable to SEM techniques. The strength of the
instrument is the energy resolution and sensitivity to very thin
layers. Monolayers can be readily detected. The detection of
sub monolayer coverage of elements is possible. High energy
resolution spectra can reveal chemical shifts in the binding
energies of electrons and can therefore give an indication of
the electronic state of the element measured. An argon
sputter gun can remove material from the surface thereby
facilitating the measurement of depth concentration profiles.
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XPS
9μm
0.1
nm
5nm hν
(x-ray)
e-
photoelectron
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Analysis facilities
Raman spectroscopy for the analysis of surface materials.
A Raman microscope setup consists of a standard
microscope, extended with an excitation laser, a
monochromator, and a sensitive detector (such as a charge-
coupled device (CCD), or photo-multiplier tube (PMT)). FT-
Raman has also been used with microscopes. Ultraviolet
microscopes and UV enhanced optics must be used when a
UV laser source is used for Raman micro spectroscopy.
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hν(laser)
hν(ir-uv)
RAMAN
0.2μm
0.2
μm
1μ
m
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Analysis: FIB and FTIR
• Focused Ion Beam. FEI’s Dual Beam System NOVA 600,
combines FIB with SEM. The combination of these two
techniques makes it ideal for micromachining. Local etching with
the ion-beam creates structures suitable for cross-sectioning
and TEM-sample preparation in a predefined part of the
substrate without damaging other parts. Cross-sectioning reveals
the underlying structure imaged by SEM. TEM-sample
preparation thins the sample down to 100 nm with minimal
damage. A 16 bit pattern generator is available to create the most
amazing structures such as 3D Photonic Crystals. Tungsten and
platinum deposition is also available.
• In an FTIR, fourier transformed infrared spectrometer , light is
reflected by or transmitted through a sample. The light interacts
with the atoms of the sample and shows shifts in the spectrum.
The shifts are characteristic for the molecules present in the
sample.
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hν(IR)
hν(IR)
FTIR
1mm 10mm
0.0
1nm
5
00nm
hν(IR)
FIB
15nm
10nm
1
0μ
m
e-e-
I+ X+
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Analysis: SEM detectors: EBIC, EBSD, ESB, STEM, EDX.
TEM detector: EDX.
• EBIC, Zeiss Merlin detector. The electron beam induced current maps the
conductivity of a sample. It can be used to identify buried
junctions and defects in semiconductor devices
• EBSD, HKL systems on the Zeiss Merlin. Electron Backscatter
Diffraction as with EDX one can use a SEM as a source of
incident electrons that are subsequently backscattered and diffracted by the
crystal lattice of small crystals that make up the surface The information
comes from a thin layer ~5 nm thick and gives information about the crystal
lattice parameters. Together with EDX it can resolve the materials at a surface
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SEM, EBSD, EBIC
1nm
1nm
500nm e-e-e-
A
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List of abbreviations
AFM-SPM atomic force microscopy – scanning probe microscopy
CA contact angle measurement
EDX/EDS energy dispersive X-ray spectroscopy
EBIC electron beam induced current
EBSD electron backscatter diffraction
EELS electron energy loss spectroscoy
EFTEM energy filtered TEM, a derivative technique of EELS.
ESCA electron spectroscopy for chemical analysis
FIB focused ion beam
FTIR Fourier transformed infrared spectrometry
GCMS gas chromatography mass spectrometry
GDMS glow discharge mass spectroscopy
HIM helium ion microscopy
ICP-OES inductive coupled plasma optical emission spectrometer
ICP-MS inductive coupled plasma ion mass spectroscopy
LEXES low energy x-ray emission spectroscopy
MP mechanical profilometry
OM optical microscopy
OP optical profilometry
RBS Rutherford back scattering
SEM scanning electron microscopy
SIMS secondary ion mass spectroscopy
(S)TEM (scanning) transmission electron microscopy
TXRF total reflections x-ray fluorescence
TOF-SIMS time of flight secondary ion mass spectroscopy
XPS x-ray photoelectron spectroscopy
XRD x-ray diffraction
XRF x-ray fluorescence
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List of operators and supervisors in cleanroom and nanolab
4 point measurement Cleanroom Eddy Ruiter 6765
4 point probe Cleanroom Robert Wijn 6770
AFM-SPM Cleanroom Robert Wijn 6770
Balance Cleanroom Eddy Ruiter 6765
Contact angle measurement Cleanroom Huib van Vossen 6769
EDX/EDS NL1.044 Mark Smithers 5922
NL1.048 Rico Keim 5915
EBIC NL1.044 Mark Smithers 5922
EBSD NL1.044 Mark Smithers 5922
EELS NL1.048 Rico Keim 5915
EFTEM NL1.048 Rico Keim 5915
Ellipsometer Cleanroom Eddy Ruiter 6765
Cleanroom Christiaan Bruinink 6399
FIB NL1.050 Henk van Wolferen 5994
HIM NL1.046 -------------------------- -------
Interferometry Cleanroom Huib van Vossen 6769
Mechanical profilometer Cleanroom Robert Wijn 6770
Optical microscopes Cleanroom Huib van Vossen 6769
NL1.027 Rico Keim 5915
Parameter analyzer Cleanroom Eddy Ruiter 6765
Reflectometer Cleanroom Huib van Vossen 6769
SEM NL1.044 Mark Smithers 5922
Cleanroom Gerard Kip 5977
TEM NL1.048 Rico Keim 5915
NL1.048 Mark Smithers 5922
XPS NL1.029 Gerard Kip 5977
XRD NL1.021 Eddy Ruiter 6765
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To do list
• Vibrating Sample Magnetometer Thijs Bolhuis
• UV Raman spectroscopy (in bio department?
• AFM types available (Martin Siekman)
• Meetmethodieken BioNanoLab (Henk)
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HIM
0.2nm
0.1
nm
1nm e-He+